WO2021193764A1 - Particule de nitrure de bore et composition de résine et récipient la comprenant - Google Patents

Particule de nitrure de bore et composition de résine et récipient la comprenant Download PDF

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Publication number
WO2021193764A1
WO2021193764A1 PCT/JP2021/012390 JP2021012390W WO2021193764A1 WO 2021193764 A1 WO2021193764 A1 WO 2021193764A1 JP 2021012390 W JP2021012390 W JP 2021012390W WO 2021193764 A1 WO2021193764 A1 WO 2021193764A1
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boron nitride
nitride particles
particles
resin
less
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PCT/JP2021/012390
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English (en)
Japanese (ja)
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建治 宮田
祐輔 佐々木
啓 久保渕
智成 宮崎
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デンカ株式会社
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Priority to JP2022510628A priority Critical patent/JPWO2021193764A1/ja
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds

Definitions

  • the present disclosure relates to boron nitride particles, and a resin composition and an inclusion body containing the boron nitride particles.
  • heat dissipation members are used to efficiently dissipate heat generated during use.
  • the heat radiating member contains, for example, ceramic particles having high thermal conductivity.
  • ceramic particles boron nitride particles having characteristics such as high thermal conductivity, high insulation, and low relative permittivity are attracting attention.
  • ammonia alkoxide having a molar ratio of ammonia / borate alkoxide of 1 to 10 and ammonia are reacted in an inert gas stream at 750 ° C. or higher within 30 seconds, and then ammonia gas or After heat treatment at 1,000 to 1,600 ° C. for 1 hour or more in an atmosphere of a mixed gas of ammonia gas and an inert gas, and further in an atmosphere of an inert gas, 1,800 to 2,200 ° C., 0.5.
  • Examples thereof include a manufacturing method in which the gas is fired in an hour or longer (see, for example, Patent Document 1).
  • one aspect of the present invention is to provide boron nitride particles having a thermal conductivity equivalent to that of the conventional one, while being easier to manufacture than the conventional one.
  • One aspect of the present invention is a boron nitride particle comprising a central portion containing low crystallinity boron nitride and a peripheral portion arranged so as to surround the central portion and containing highly crystalline boron nitride.
  • the average circularity of the boron nitride particles may be 0.8 or more.
  • Another aspect of the present invention is a resin composition containing a resin and the above-mentioned boron nitride particles.
  • Another aspect of the present invention is an accommodating body including the above-mentioned boron nitride particles and a container for accommodating the boron nitride particles.
  • boron nitride particles having a thermal conductivity equivalent to that of the conventional one, while being more easily produced than the conventional one.
  • One embodiment of the present invention is a boron nitride particle comprising a central portion containing low crystalline boron nitride and a peripheral portion arranged so as to surround the central portion and containing highly crystalline boron nitride. ..
  • high crystallinity is derived from the h-BN (0002) plane in the range of 1 to 4 nm -1 on the reciprocal lattice space in the FFT image of the boron nitride particles obtained by the following method. It means a state in which a bright spot (peak) is present due to the periodicity of the above, and “low crystallinity” means a state in which the bright spot (peak) does not exist.
  • the existence of a bright spot (peak) means that the intensity S after subtracting the background by the B-spline method in the range of 1 to 4 nm -1 on the reciprocal lattice space is 15 times or more the noise intensity N. It means that there is a point that becomes.
  • the noise intensity N is defined as the value of the standard deviation in the range of more than 4 nm -1 and 6 nm -1 or less on the reciprocal lattice space after performing background processing by the B-spline method.
  • the bright spots (peaks) include those having fluctuations in the wave number direction or the circumferential direction.
  • the intensity S is preferably 20 times or more, more preferably 23 times the noise intensity N in the range of 1 to 4 nm -1 on the reciprocal lattice space. As mentioned above, there may be a point that is more preferably 25 times or more.
  • FFT image acquisition method First, using a transmission electron microscope (for example, "JEM-2100” manufactured by JEOL Ltd.), a TEM image of 400,000 times that of boron nitride particles is obtained under the following conditions. Objective lens aperture: ⁇ 120 ⁇ m Condenser lens aperture: ⁇ 150 ⁇ m Recording medium: "Orisus SC1000A1" manufactured by AMETEK Bining: 2 Exposure time: 0.5 seconds In addition, image analysis software (for example, "GMS3" manufactured by AMETEC) is used for TEM observation and FFT analysis described later. Subsequently, an FFT analysis is performed on a region of 8.556 nm square in the obtained TEM image, and an FFT image of 256 ⁇ 256 pixels is acquired.
  • a transmission electron microscope for example, "JEM-2100” manufactured by JEOL Ltd.
  • the diameter of the central portion of the boron nitride particles may be, for example, 0.1d or more, 0.15d or more, or 0.2d or more, and 0.6d or less, where d is the particle size of the boron nitride particles. , 0.5 or less, 0.4d or less, 0.35d or less, or 0.3d or less.
  • the diameter of the central portion in the boron nitride particles may be, for example, 1 nm or more, 5 nm or more, 10 nm or more, 20 nm or more, or 30 nm or more, and may be 400 nm or less, 300 nm or less, 200 nm or less, or 100 nm or less.
  • the diameter of the central portion in the boron nitride particles is derived from the h-BN (0002) plane in the “highly crystalline” portion defined as described above, that is, in the range of 1 to 4 nm -1 on the reciprocal lattice space. It means the diameter of the part where the bright spot (peak) exists due to the periodicity of.
  • the thickness of the peripheral portion in the boron nitride particles may be, for example, 0.3d or more, 0.33d or more, or 0.35d or more, and 0.45d or more, where d is the particle size of the boron nitride particles. Hereinafter, it may be 0.43d or less, or 0.4d or less.
  • the diameter of the central portion in the boron nitride particles may be, for example, 5 nm or more, 10 nm or more, 20 nm or more, 40 nm or more, or 60 nm or more, and may be 450 nm or less, 300 nm or less, 200 nm or less, or 100 nm or less.
  • the thickness of the peripheral portion in the boron nitride particles is the h-BN (0002) plane in the “low crystallinity” portion defined as described above, that is, in the range of 1 to 4 nm -1 on the reciprocal lattice space. It means the thickness of the part where there is no bright spot (peak) due to the periodicity of origin.
  • the average particle size of the boron nitride particles is preferably 0.01 ⁇ m or more, 0.05 ⁇ m or more, 0.1 ⁇ m or more, or 0.15 ⁇ m from the viewpoint of suppressing an increase in viscosity when the boron nitride particles and the resin are mixed.
  • the heat radiating member containing the boron nitride particles hereinafter, also simply referred to as “radiating member”.
  • the average particle size of the boron nitride particles is measured by the following procedure. Distilled water is used as a dispersion medium for dispersing the boron nitride particles, and sodium hexametaphosphate is used as a dispersant to prepare a 0.125 mass% sodium hexametaphosphate aqueous solution. Boron nitride particles are added to this aqueous solution at a ratio of 0.1 g / 80 mL, and ultrasonic dispersion is performed at 80% AMPLITUDE (amplitude) for 1 minute using an ultrasonic homogenizer (for example, "US-300E" manufactured by Nissei Tokyo Office).
  • an ultrasonic homogenizer for example, "US-300E" manufactured by Nissei Tokyo Office.
  • a dispersion of boron nitride particles is prepared by performing this once every 30 seconds. This dispersion is separated while stirring at 60 rpm, and the volume-based particle size distribution is measured by a laser diffraction / scattering method particle size distribution measuring device (for example, “LS-13 320” manufactured by Beckman Coulter). At this time, 1.33 is used as the refractive index of water, and 1.7 is used as the refractive index of the boron nitride particles. From the measurement results, the average particle size is calculated as a particle size (median diameter, d50) of 50% of the cumulative value of the cumulative particle size distribution. The average particle size measured in this way is considered to be the average particle size of the boron nitride particles including the primary particles of the boron nitride particles and the particles (secondary particles) in which the primary particles are aggregated. ..
  • Boron nitride particles preferably have a spherical shape or a shape close to a spherical shape from the viewpoint of improving the filling property when manufacturing the heat radiating member and making the characteristics (thermal conductivity, dielectric constant, etc.) of the heat radiating member isotropic. have.
  • the average circularity of the boron nitride particles is preferably 0.8 or more, 0.82 or more, 0.84 or more, 0.86 or more, 0.88 or more, 0.90 or more, 0.91. As mentioned above, it may be 0.92 or more, 0.93 or more, or 0.94 or more.
  • the boron nitride particles as described above can be obtained by intentionally stopping the crystal growth of boron nitride in an incomplete state.
  • the crystal growth gradually progresses from the peripheral portion to the central portion of the particles, and the boron nitride particles obtained by stopping the crystal growth of boron nitride in an incomplete state are used.
  • the boron nitride contained in the peripheral portion has high crystallinity, while the boron nitride contained in the central portion has low crystallinity.
  • the above-mentioned boron nitride particles are nitrided by, for example, the first step of reacting boric acid ester and ammonia at 750 to 1400 ° C. to obtain a precursor of the boron nitride particles, and heating the precursor at 1000 to 1600 ° C. It is obtained by a production method comprising a second step of obtaining boron particles.
  • a reaction tube for example, a quartz tube installed in a resistance heating furnace is heated to raise the temperature to 750 to 1500 ° C.
  • the boric acid ester is introduced into the reaction tube by passing the inert gas through the liquid boric acid ester and then introducing it into the reaction tube.
  • ammonia gas is introduced directly into the reaction tube.
  • the inert gas include rare gases such as helium, neon and argon, and nitrogen gas.
  • the borate ester may be, for example, an alkyl borate ester, preferably trimethyl borate.
  • the molar ratio of the amount of ammonia introduced to the amount of boric acid introduced may be, for example, 1 or more and 10 or less.
  • the introduced boric acid ester and ammonia react in a heated reaction tube to produce a precursor of boron nitride particles.
  • This precursor contains amorphous boron nitride and may be, for example, a white powder.
  • a part of the generated precursor adheres to the inside of the reaction tube, but most of the precursor is sent to the recovery container attached to the tip of the reaction tube by the inert gas or unreacted ammonia gas and recovered.
  • the time (reaction time) for reacting the boric acid ester with ammonia in the first step is preferably within 30 seconds.
  • the reaction time is the time during which the boric acid ester and ammonia stay in the portion of the reaction tube heated to 750 to 1400 ° C. (heated portion), and the gas flow rate when introducing the boric acid ester and ammonia and resistance heating. It can be adjusted by the length of the reaction tube installed in the furnace (the length of the heated portion of the reaction tube).
  • the precursor obtained in the first step is placed in another reaction tube (for example, an alumina tube) installed in the resistance heating furnace, and nitrogen gas and ammonia gas are separately placed in the reaction tube. Introduce.
  • the gas introduced at this time may be only ammonia gas.
  • the flow rates of nitrogen gas and ammonia gas may be appropriately adjusted so that the reaction time becomes a desired value, respectively. For example, the higher the flow rate of ammonia gas, the shorter the reaction time.
  • the reaction tube is heated to 1000 to 1600 ° C.
  • the heating time may be, for example, 1 hour or more and 10 hours or less.
  • the crystallization of boron nitride in the precursor is promoted to obtain boron nitride particles.
  • all the boron nitride in the precursor is not crystallized, and low crystalline boron nitride remains inside the boron nitride particles.
  • the boron nitride particles obtained in the second step are heated at 1800 ° C. or higher (conventional step, which was conventionally carried out to promote the crystal growth of boron nitride). Does not have. That is, in this production method, the desired boron nitride particles are obtained in a state of incomplete crystal growth after heating in the second step.
  • the boron nitride particles obtained in the second step are subjected to 1700 ° C. or higher, 1600 ° C. or higher, 1500 ° C. or higher, 1400 ° C. or higher, 1300 ° C. or higher, 1200 ° C. or higher, 1100.
  • °C or more 1000 °C or more, 900 °C or more, 800 °C or more, 700 °C or more, 600 °C or more, 500 °C or more, 400 °C or more, 300 °C or more, 200 °C or more, 100 °C or more, 50 °C or more, 40 °C or more Or, it does not have to be provided with a step of heating at 30 ° C. or higher.
  • the above-mentioned boron nitride particles are suitably used for, for example, a heat radiating member.
  • the boron nitride particles are used, for example, in the form of a resin composition mixed with a resin.
  • another embodiment of the present invention is a resin composition containing the resin and the above-mentioned boron nitride particles. This resin composition is suitably used as a heat radiating member.
  • the content of the above-mentioned boron nitride particles is preferably 30% by volume or more, based on the total volume of the resin composition, from the viewpoint of improving the thermal conductivity of the resin composition and easily obtaining excellent heat dissipation performance. It is preferably 40% by volume or more, more preferably 50% by volume or more, and preferably 85% by volume or less, more preferably 85% by volume or less, from the viewpoint of suppressing the generation of voids during molding and the decrease in insulating property and mechanical strength. It is 80% by volume or less, more preferably 70% by volume or less.
  • the resin examples include epoxy resin, silicone resin, silicone rubber, acrylic resin, phenol resin, melamine resin, urea resin, unsaturated polyester, fluororesin, polyimide, polyamideimide, polyetherimide, polybutylene terephthalate, polyethylene terephthalate, and the like.
  • the content of the resin may be 15% by volume or more, 20% by volume or more, or 30% by volume or more, based on the total volume of the resin composition, and is 70% by volume or less, 60% by volume or less, or 50% by volume. It may be:
  • the resin composition may further contain a curing agent that cures the resin.
  • the curing agent is appropriately selected depending on the type of resin.
  • examples of the curing agent include phenol novolac compounds, acid anhydrides, amino compounds, and imidazole compounds.
  • the content of the curing agent may be, for example, 0.5 parts by mass or more or 1.0 part by mass or more, and may be 15 parts by mass or less or 10 parts by mass or less with respect to 100 parts by mass of the resin.
  • Boron nitride particles can be distributed in a container, for example. That is, another embodiment of the present invention is an accommodating body including the above-mentioned boron nitride particles and a container for accommodating the boron nitride particles.
  • the container may have a shape capable of accommodating boron nitride particles, and may be, for example, a bag, a box, a bottle, a can, or the like.
  • Example 1 (Preparation of boron nitride particles)
  • the reaction tube (quartz tube) installed in the resistance heating furnace was heated to raise the temperature to 1150 ° C.
  • trimethyl borate was introduced into the reaction tube by passing nitrogen gas through trimethyl borate and then introducing it into the reaction tube.
  • ammonia gas was introduced directly into the reaction tube.
  • the molar ratio of the amount of ammonia introduced to the amount of trimethyl borate introduced was 4.5.
  • trimethyl borate was reacted with ammonia to obtain a precursor (white powder) of boron nitride particles.
  • the reaction time was 10 seconds.
  • the precursor obtained in the first step is placed in another reaction tube (alumina tube) installed in the resistance heating furnace, and nitrogen gas 10 L / min and ammonia gas 15 L. Each was introduced into the reaction tube separately at a flow rate of / min. Then, the reaction tube was heated at 1500 ° C. for 2.5 hours. As a result, boron nitride particles were obtained.
  • alumina tube alumina tube
  • FIG. 1 shows a TEM bright-field image (magnification: 100,000 times) of the obtained boron nitride particles as a whole.
  • FIG. 2 shows a TEM dark-field image of the peripheral portion S of the boron nitride particles shown in FIG. 1 observed at a magnification of 400,000.
  • FIG. 4 FFT analysis was performed on the other regions S2 to S5 in the peripheral portion S of the boron nitride particles in the same manner as in the region S1.
  • FIGS. 4 and 5 bright spots (peaks) due to periodicity derived from the h-BN (0002) plane were confirmed in the range of 1 to 4 nm -1 on the reciprocal lattice space. That is, it was confirmed that the regions S2 to S5 in the peripheral portion S of the boron nitride particles were also composed of highly crystalline boron nitride.
  • FIG. 6 shows a TEM dark-field image of the central portion C of the boron nitride particles shown in FIG. 1 observed at a magnification of 400,000.
  • FFT analysis was also performed on the regions C1 to C4 in the central portion C of the boron nitride particles in the same manner as in the region S1.
  • no bright spot (peak) due to periodicity derived from the h-BN (0002) plane was confirmed in the range of 1 to 4 nm -1 on the reciprocal lattice space. That is, it was confirmed that the regions C1 to C4 in the central portion C of the boron nitride particles are composed of low crystallinity boron nitride.
  • the graphs shown in FIGS. 3 (b), 5 and 7 are graphs showing the intensity after subtracting the background by the B-spline method. Further, from the graphs shown in FIGS. 5 and 7 of FIG. 3B, the maximum intensity (relative intensity) Smax in the range of 1 to 4 nm -1 on the reciprocal lattice space for each of the regions S1 to S5 and C1 to C4. The noise intensity (standard deviation in the range of more than 4 nm -1 and 6 nm -1 or less on the reciprocal lattice space) N and their ratio (Smax / N) were obtained. The results are shown in Table 1.
  • the obtained boron nitride particles contain highly crystalline boron nitride in the peripheral portion (the region where the above-mentioned bright spot (peak) can be confirmed is dominant), and the central portion is low. It was found that crystalline boron nitride was contained (the region where the above-mentioned bright spot (peak) could not be confirmed was dominant).
  • the diameter of the central portion was about 40 nm, and the thickness of the peripheral portion was about 50 nm.
  • Distilled water was used as a dispersion medium for dispersing the boron nitride particles, and sodium hexametaphosphate was used as a dispersant to prepare a 0.125 mass% sodium hexametaphosphate aqueous solution.
  • Boron nitride particles obtained at a ratio of 0.1 g / 80 mL are added to this aqueous solution, and ultrasonic dispersion is performed at 80% AMPLITUDE (amplitude) by an ultrasonic homogenizer (“US-300E” manufactured by Nissei Tokyo Office).
  • a dispersion of boron nitride particles was prepared by performing the procedure once every minute and 30 seconds.
  • This dispersion was separated while stirring at 60 rpm, and the volume-based particle size distribution was measured with a laser diffraction / scattering method particle size distribution measuring device (“LS-13 320” manufactured by Beckman Coulter). At this time, 1.33 was used as the refractive index of water, and 1.7 was used as the refractive index of the boron nitride particles. From the measurement results, the average particle size was calculated as a particle size (median diameter, d50) of 50% of the cumulative value of the cumulative particle size distribution. The average particle size of the obtained boron nitride particles was 510 nm.
  • Comparative Example 1 After the second step of Example 1, the boron nitride particles were placed in a boron nitride crucible and heated in an induction heating furnace at 2000 ° C. for 5 hours in the same manner as in Example 1. Boron nitride particles for comparison were obtained. That is, in Comparative Example 1, comparative boron nitride particles were obtained by a conventional production method.
  • the thermal conductivity of the boron nitride particles obtained in Example 1 and the comparative boron nitride particles obtained in Comparative Example 1 was measured by the following procedure. 40 parts by mass of boron nitride particles with respect to a mixture of 100 parts by mass of naphthalene type epoxy resin (manufactured by DIC, "HP4032”) and 10 parts by mass of imidazoles (manufactured by Shikoku Kasei Co., Ltd., "2E4MZ-CN)) as a curing agent. A resin composition was obtained by mixing so as to be%.
  • the specific gravity B (kg / m 3 ) of the measurement sample was measured by the Archimedes method.
  • Example 1 the boron nitride particles obtained in Example 1 showed 1.13 W / (m ⁇ K), and the comparative boron nitride particles obtained in Comparative Example 1 showed 1.12 W / (m ⁇ K). rice field.
  • Example 1 although the step of Comparative Example 1 (the step carried out by the conventional manufacturing method) of heating at 2000 ° C. for 5 hours in a nitrogen atmosphere was omitted, it was different from that of Comparative Example 1. Boron nitride particles having the same thermal conductivity could be obtained.

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Abstract

Selon un aspect de l'invention, la présente invention concerne une particule de nitrure de bore qui comprend une partie de noyau, ladite partie de noyau contenant du nitrure de bore cristallin faible, et une partie de coque, ladite partie de coque étant disposée de manière à entourer la partie de noyau et contenant du nitrure de bore cristallin élevé.
PCT/JP2021/012390 2020-03-26 2021-03-24 Particule de nitrure de bore et composition de résine et récipient la comprenant WO2021193764A1 (fr)

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Citations (4)

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US20020155052A1 (en) * 2001-04-24 2002-10-24 Paine Robert T. Organoboron route and process for preparation of boron nitride
CN1931719A (zh) * 2005-12-01 2007-03-21 华中师范大学 一种六方氮化硼纳米微球及合成方法和应用
JP2010180066A (ja) * 2009-02-03 2010-08-19 National Institute For Materials Science 窒化ホウ素球状ナノ粒子とその製造方法
JP2011056438A (ja) * 2009-09-11 2011-03-24 Hokkaido Univ 金属担持結晶性窒化ボロン複合材料、その製造方法およびその利用

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020155052A1 (en) * 2001-04-24 2002-10-24 Paine Robert T. Organoboron route and process for preparation of boron nitride
CN1931719A (zh) * 2005-12-01 2007-03-21 华中师范大学 一种六方氮化硼纳米微球及合成方法和应用
JP2010180066A (ja) * 2009-02-03 2010-08-19 National Institute For Materials Science 窒化ホウ素球状ナノ粒子とその製造方法
JP2011056438A (ja) * 2009-09-11 2011-03-24 Hokkaido Univ 金属担持結晶性窒化ボロン複合材料、その製造方法およびその利用

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Title
TANG, C. ET AL.: "Synthetic routes and formation mechanisms of spherical boron nitride nanoparticles", ADVANCED FUNCTIONAL MATERIALS, vol. 18, no. 22, 30 October 2008 (2008-10-30), pages 3653 - 3661, XP001517179, DOI: 10.1002/adfm.200800493 *
XU FEN, XIE YI, ZHANG XU, ZHANG SHUYUAN, LIU XIANMING, TIAN XIAOBO: "Synergic Nitrogen Source Route to Inorganic Fullerene-like Boron Nitride with Vessel, Hollow Sphere, Onion, and Peanut Nanostructures", INORGANIC CHEMISTRY, vol. 43, 18 December 2003 (2003-12-18), pages 822 - 829, XP055861834, DOI: 10.1021/ic0348751 *

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